CN109772295A - A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application - Google Patents
A kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of bismuth tungstates to modify antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application, belong to photoelectrocatalysis field, composite photoelectric catalysis electrode is a kind of electrode formed including bismuth tungstate and antimony-doped stannic oxide, wherein the molar ratio of stannic oxide and bismuth tungstate is 9:0.1-2, its preparation step includes: to synthesize bismuth tungstate powder using hydrothermal synthesis method, after high-temperature process, bismuth tungstate is added when preparing tin antimony collosol and gel, composite photoelectric catalysis electrode is prepared using collosol and gel coating thermal decomposition method.Photoelectric properties experiment shows that the composite photoelectric catalysis electrode possesses higher catalytic activity and photoelectric current relative to antimony-doped stannic oxide electrode, has potential application prospect in Solar use and field of waste water treatment.
Description
Technical field
The present invention relates to a kind of bismuth tungstates to modify antimony-doped stannic oxide composite photoelectric catalysis electrode, preparation method and application,
Belong to photoelectrocatalysielectrode electrode technical field.
Background technique
Industrial production and agricultural development produce the waste water of the largely hardly degraded organic substance containing persistence, cause sternly to environment
Heavily contaminated.Traditional waste water treatment process is mainly biological treatment, can not completely remove pesticide or antibiotic from water body.
Titanium-based antimony-doped stannic oxide electrode works well to treatment of Organic Wastewater, have it is cheap and easy to get, catalytic performance is excellent, electric conductivity and
The features such as chemical stability is good is widely used in electro-catalysis field of waste water treatment.But existing antimony-doped stannic oxide electrode photoelectric is urged
Change low efficiency, the antimony-doped stannic oxide electrode for how obtaining high catalytic efficiency has become the research hotspot of field of waste water treatment.
Summary of the invention
Aiming at the shortcomings in the prior art, the present invention provides a kind of bismuth tungstate modification antimony-doped stannic oxide composite photoelectrics to urge
Polarizing electrode, preparation method and application, to promote antimony-doped stannic oxide electrode to the drop of persistence hardly degraded organic substance waste water ability
Solution ability.
In order to solve the above-mentioned technical problem, technical scheme is as follows:
A kind of preparation method of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, includes the following steps:
S1, water-soluble bismuth salt is dissolved in the water, is stirred evenly, then 20~40min of ultrasound, obtain solution A；
Water-soluble tungstates is dissolved in ethylene glycol, is stirred evenly, then 20~40min of ultrasound, obtains solution B；
Solution B is instilled in solution A under ultrasound condition, is mixed, solution C is obtained；
Solution C is transferred to hydrothermal reaction kettle, 8~20h is reacted under the conditions of 120~200 DEG C, then product is taken out, it is cold
But to after room temperature, filter, and successively washing, alcohol are washed repeatedly, 10~12h then dried at 60~80 DEG C, obtain bismuth tungstate (with
Bi2WO6Meter)；
S2, citric acid, dihydric alcohol, Tin tetrachloride pentahydrate, antimony trichloride and bismuth tungstate are pressed into (115~135): (32~
38) molar ratio mixing: 9:1:(0.1~2), obtains sol-gel precursor；
S3, the sol-gel precursor obtained in S2 is brushed on Titanium base, then be dried, thermal oxidation, so
After to be repeated in brushing, drying and thermal oxidation step multiple, finally anneal under the conditions of 450~650 DEG C 1.5~3.5h,
It obtains bismuth tungstate and modifies antimony-doped stannic oxide composite photoelectric catalysis electrode.
Optionally, in S1, water-soluble bismuth salt is dissolved in the water, stirs 5-15min, preferably 10min, then ultrasound 20
~40min obtains solution A；
Water-soluble tungstates is dissolved in ethylene glycol, stir 5-15min, preferably 10min, then ultrasound 20~
40min obtains solution B.
Further, in S1, the water solubility bismuth salt is five water bismuth nitrates；The water solubility tungstates is tungstate dihydrate acid
Sodium.
Further, in S1, the molar ratio of sodium tungstate is (2~2.5) in bismuth nitrate and solution B in solution A: 1, further
For (2.2-2.4): 1.
Further, in S1, it is 0.3~0.5mL/min that solution B instills the speed in solution A under ultrasound condition.Ultrasound
Under the conditions of be more favorable for solution dispersion, meanwhile, solution A and solution B reaction be metathesis reaction, have precipitating generate, coutroi velocity
It can control product generating rate, and then control the pattern and partial size of product.
Further, in S1, alcohol is washed finger and is cleaned using ethyl alcohol as cleansing medium to product.
Further, in S2, the bismuth tungstate is that the bismuth tungstate in bismuth tungstate and/or S1 in S1 is obtained by calcination processing
The bismuth tungstate obtained.
Further, the calcination processing process are as follows: under the conditions of the bismuth tungstate in S1 is placed in 350-550 DEG C calcine 2~
3h.Preferably, 2~3h is calcined under the conditions of 450 DEG C, applicants have found that, it controls at such a temperature, the wolframic acid finally obtained
Bismuth photocatalysis effect is preferable.Suitable calcination temperature can improve the specific surface area and crystallinity of bismuth tungstate, and adjustment absorbs band edge,
Increase the absorption region to visible light.
Further, in S2, the dihydric alcohol includes ethylene glycol.
Further, in S3, when dry, Titanium base is placed in infrared oven and is carried out, optionally, at 115-190 DEG C
Under the conditions of dry 8-22min.
Further, in S3, brushing, drying and thermal oxidation step 3~25 time, generally 8~20 times are repeated in,
It is further 12~16 times.When low repetition, electrode load active material is few, and electric conductivity and catalytic performance are bad；But again
Again number is excessive, and continually so that the structure of matter is destroyed, electrode performance is reduced for high temperature drying and thermal oxide meeting.
Further, in S3, thermal oxidation method are as follows: 10~20min of thermal oxide at 550 DEG C in Muffle furnace.
Preferably, in S3, it is further 520~580 DEG C that annealing temperature, which is 450~650 DEG C,.
Further, in S3, the Titanium base is by titanium exemplar successively after polishing, alkali cleaning oil removing, acid etching technique, cleaning
It obtains.
Preferably, the Titanium base is tabular.
Further, the bruting process is successively to be polished with 400 mesh, 800 mesh, 1200 mesh sand paper titanium exemplar,
Optionally, using SiC sand paper.
The present invention also provides a kind of bismuth tungstates to modify antimony-doped stannic oxide composite photoelectric catalysis electrode, by making as described above
Preparation Method is made.
The present invention also provides the modification antimony-doped stannic oxide composite photoelectrics of bismuth tungstate made of preparation method as described above to urge
Polarizing electrode or bismuth tungstate as described above modification antimony-doped stannic oxide composite photoelectric catalysis electrode are in treatment of Organic Wastewater field
Using.
Further, application of the bismuth tungstate photocatalyst in photochemical catalytic oxidation waste water in hardly degraded organic substance.
Further, the bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode is in photoelectrocatalysioxidization oxidization waste water
Application in middle hardly degraded organic substance.
In the application, citric acid is a kind of tricarboxylic acid, esterification can occur with dihydric alcohol, generate the netted of polymerization
The structural stability of gel compound can be improved in high polymer.Meanwhile citric acid can be used as metal ion network mixture, facilitate
It is dispersed in metal ion in collosol and gel.
Applicants have found that stannic oxide is a kind of n-type semiconductor, forbidden bandwidth is about 3.5eV, and photoresponse is poor.Tungsten
Sour bismuth forbidden bandwidth is about 2.8eV, is a kind of ideal visible light catalyst, however, photo-generate electron-hole pairs is quick compound
So that its photocatalysis effect is not significant.Bismuth tungstate is modified and is urged in formation composite photoelectric on antimony-doped stannic oxide electrode by the present invention
Polarizing electrode improves response of the combination electrode to light, simultaneously while improving former antimony-doped stannic oxide electrode electrocatalysis characteristic
Light induced electron and hole are efficiently separated, photocatalysis effect is improved, reaches electrical enhanced photocatalysis
Purpose, improve to the treatment effeciency of the waste water of hardly degraded organic substance containing persistence.In addition, the present invention, which is equivalent to, provides a kind of powder
Powder semiconductor catalyst can be made into optoelectronic pole to be used for photoelectrocatalysis by the carrying method of last catalyst.
Bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode of the invention is by bismuth tungstate and antimony-doped stannic oxide
Composition.Bismuth tungstate is modified so that electrode electrocatalysis characteristic is improved, and photoresponse enhancing, photoelectric current increases, while being powered on outside
Off field photo-generate electron-hole is quickly and effectively separated, to effectively increase electrode to the treatment effeciency of organic matter, Ke Yiguang
It is general to be applied to wastewater treatment.
Detailed description of the invention
Fig. 1 penetrates for the X of bismuth tungstate prepared by the present invention and bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode
Ray diffraction diagram spectrum；
Fig. 2 is that a kind of bismuth tungstate prepared by the present invention is modified under antimony-doped stannic oxide composite photoelectric catalysis electrode open circuit potential
Photocurrent-time figure；
Fig. 3 is that bismuth tungstate prepared by the present invention modifies antimony-doped stannic oxide composite photoelectric catalysis electrode at 0.8V (vs.SCE)
Photocurrent-time figure under bias.
Fig. 4 is that bismuth tungstate prepared by embodiment 1 modifies antimony-doped stannic oxide composite photoelectric catalysis electrode to Ciprofloxacin
Degradation changes over time curve.
Specific embodiment
Below with reference to embodiment and attached drawing, invention is further described in detail.
Embodiment 1
In the present embodiment, bismuth tungstate modify antimony-doped stannic oxide composite photoelectric catalysis electrode the preparation method is as follows:
S1, five water bismuth nitrate of 2mmol is dissolved in 30mL water, stirs ultrasound 30min, obtain solution A；
1mmol tungstate dihydrate acid sodium is dissolved in 20mL ethylene glycol, ultrasound 30min is stirred, obtains solution B；
Solution B is instilled in solution A under ultrasound condition with the rate of 0.3mL/min and is mixed to get solution C；
Solution C is transferred to hydrothermal reaction kettle, 12h is reacted at 180 DEG C, is cooled to room temperature after taking-up, the production that will be obtained
Object filters, and is washed 3 times with water and ethyl alcohol respectively, then the dry 12h at 80 DEG C, obtains bismuth tungstate (with Bi2WO6Meter), product is put
It is placed in crucible, calcines 3h at 450 DEG C；
S2, citric acid, ethylene glycol, Tin tetrachloride pentahydrate, antimony trichloride and the bismuth tungstate are pressed into 130:30:9:1:
0.5 molar ratio is at sol-gel precursor；
S3, titanium plate is cut into size 2.0cm × 2.0cm, is successively polished using 400 mesh, 800 mesh, 1200 mesh sand paper,
Oil removing 1h in 10wt% sodium hydroxide solution；Then the heating etching 2h in 10wt% oxalic acid solution；It finally rinses well, is placed in
It is saved backup in ultrapure water, obtains Titanium base；
The sol-gel precursor of above-mentioned preparation is brushed on Titanium base, and 10min then is dried in infrared oven,
Thermal oxidation 10min is carried out at 550 DEG C in Muffle furnace, is repeated in brushing, drying and thermal oxidation step 12 time, most
Anneal under the conditions of 550 DEG C 2h afterwards, obtains bismuth tungstate and modifies antimony-doped stannic oxide composite photoelectric catalysis electrode.
Fig. 1 is that bismuth tungstate powder (a) prepared by the embodiment of the present invention 1 and bismuth tungstate modify antimony-doped stannic oxide complex light
The X ray diffracting spectrum of electro catalytic electrode (b) schemes the crystal faces such as (131), (200) (202) of high-visible bismuth tungstate in a, schemes b
In have the diffraction maximum of apparent stannic oxide (110) and (101) crystal face, may be smaller due to the relative amount of bismuth tungstate, do not have
Apparent bismuth tungstate diffraction maximum.
Fig. 2 is photocurrent-time curve figure of the combination electrode under open-circuit voltage prepared by embodiment 1, specific to test
Condition are as follows: standard three electrode system is used, electrode prepared by embodiment 1 is working electrode, and saturated calomel electrode is reference electrode,
Platinum is to test current-time curvel under open circuit potential in 0.5mol/L metabisulfite solution to electrode.As seen from the figure, transient state photoelectricity
Stream reaches as high as 83 μ A/cm2, 70 μ A/cm are about reduced to after 30s2, recombination rate is about 15.6%.Under same test condition, do not repair
The antimony-doped stannic oxide electrode of decorations, transient photocurrents are 36 μ A/cm2。
Fig. 3 is photocurrent-time curve figure of the prepared combination electrode under 0.8V (vs.SCE) bias, specific to test
Condition are as follows: use standard three electrode system, electrode prepared by embodiment 1 is working electrode, and saturated calomel electrode is reference, and platinum is
To electrode, current-time curvel is tested under 0.8V (vs.SCE) bias in 0.5mol/L metabisulfite solution.As seen from the figure, outside
Under biasing 0.8V, photoelectric current is up to 280-350 μ A/cm2, unmodified antimony-doped stannic oxide electrode, photoelectricity under this condition
Stream is about 140 μ A/cm2。
Embodiment 2
Bismuth tungstate to prepare in testing example 1 modifies antimony-doped stannic oxide composite photoelectric catalysis electrode to Ciprofloxacin
Degradation effect, tested with the following method:
Compound concentration is the Ciprofloxacin simulated wastewater 100mL of 30mg/L, and addition 25g/L sodium sulphate, will as electrolyte
The electrode prepared in embodiment 1 is as anode, and for stainless steel as cathode, control current density is 15mA/cm2.It stirs in the dark
30min is mixed, is powered while opening light source, is sampled every 15min, Ciprofloxacin Concentration is measured, records data.Fig. 4 is to implement
The composite photoelectric catalysis electrode of example 1 changes over time curve to the degradation of Ciprofloxacin.The results show that after light irradiates 60min,
Electrode prepared by embodiment 1 can remove 90% or more Ciprofloxacin, and unmodified antimony-doped stannic oxide electrode is in similarity condition
Under be about 85% to the degradation rate of Ciprofloxacin.
To sum up, composite photoelectric catalysis electrode of the invention possesses higher catalytic activity relative to antimony-doped stannic oxide electrode
With the absorption to light, there is potential application prospect in Solar use and field of waste water treatment.
Above said content is that a further detailed description of the present invention in conjunction with specific preferred embodiments, is not
Whole or unique embodiment, those of ordinary skill in the art are by reading description of the invention to technical solution of the present invention
Any equivalent transformation taken, all are covered by the claims of the invention.
Claims (10)
1. a kind of preparation method of bismuth tungstate modification antimony-doped stannic oxide composite photoelectric catalysis electrode, which is characterized in that including such as
Lower step:
S1, water-soluble bismuth salt is dissolved in the water, is stirred evenly, then 20~40min of ultrasound, obtain solution A；
Water-soluble tungstates is dissolved in ethylene glycol, is stirred evenly, then 20~40min of ultrasound, obtains solution B；
Solution B is instilled in solution A under ultrasound condition, is mixed, solution C is obtained；
Solution C is transferred to hydrothermal reaction kettle, 8~20h is reacted under the conditions of 120~200 DEG C, then product is taken out, is cooled to
It after room temperature, filters, and successively washing, alcohol are washed repeatedly, then dry 10~12h at 60~80 DEG C, obtains bismuth tungstate；
S2, citric acid, dihydric alcohol, Tin tetrachloride pentahydrate, antimony trichloride and bismuth tungstate are pressed into (115~135): (32~38):
9:1:(0.1~2) molar ratio mixing, obtain sol-gel precursor；
S3, the sol-gel precursor obtained in S2 is brushed on Titanium base, then is dried, thermal oxidation, then according to
Secondary brushing, drying and the thermal oxidation step of repeating is multiple, and finally anneal under the conditions of 450~650 DEG C 1.5~3.5h, obtains
Bismuth tungstate modifies antimony-doped stannic oxide composite photoelectric catalysis electrode.
2. preparation method according to claim 1, which is characterized in that in S1, the water solubility bismuth salt is five water bismuth nitrates；
The water solubility tungstates is tungstate dihydrate acid sodium.
3. preparation method according to claim 1, which is characterized in that in S1, wolframic acid in bismuth nitrate and solution B in solution A
The molar ratio of sodium is (2~2.5): 1.
4. preparation method according to claim 1, which is characterized in that in S1, solution B instills solution A under ultrasound condition
In speed be 0.3~0.5mL/min.
5. preparation method according to any one of claims 1 to 4, which is characterized in that in S2, the bismuth tungstate is in S1
Bismuth tungstate in bismuth tungstate and/or S1 passes through the bismuth tungstate that calcination processing obtains.
6. preparation method according to claim 5, which is characterized in that the calcination processing process are as follows: by the wolframic acid in S1
Bismuth calcines 2~3h under the conditions of being placed in 350-550 DEG C.
7. preparation method according to any one of claims 1 to 4, which is characterized in that in S2, the dihydric alcohol includes second two
Alcohol.
8. preparation method according to any one of claims 1 to 4, which is characterized in that in S3, be repeated in brushing, drying
It is further 12~16 times with thermal oxidation step 3~25 time, generally 8~20 times.
9. a kind of bismuth tungstate modifies antimony-doped stannic oxide composite photoelectric catalysis electrode, which is characterized in that by such as claim 1~8
Described in any item preparation methods are made.
10. bismuth tungstate made of preparation method as described in any one of claims 1 to 8 modifies antimony-doped stannic oxide composite photoelectric
Catalysis electrode or bismuth tungstate as claimed in claim 9 modification antimony-doped stannic oxide composite photoelectric catalysis electrode are at organic wastewater
The application in reason field.
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